EP0265619B1 - Verfahren zur Herstellung ebener Flächen durch Silylation - Google Patents

Verfahren zur Herstellung ebener Flächen durch Silylation Download PDF

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Publication number
EP0265619B1
EP0265619B1 EP87112330A EP87112330A EP0265619B1 EP 0265619 B1 EP0265619 B1 EP 0265619B1 EP 87112330 A EP87112330 A EP 87112330A EP 87112330 A EP87112330 A EP 87112330A EP 0265619 B1 EP0265619 B1 EP 0265619B1
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EP
European Patent Office
Prior art keywords
insulator
silylation
photoactive
photoresist
etching
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Expired - Lifetime
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EP87112330A
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English (en)
French (fr)
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EP0265619A3 (en
EP0265619A2 (de
Inventor
Garth Alwyn Brooks
Nancy Anne Greco
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International Business Machines Corp
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International Business Machines Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
    • H01L21/02164—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon oxide, e.g. SiO2
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/16—Coating processes; Apparatus therefor
    • G03F7/162—Coating on a rotating support, e.g. using a whirler or a spinner
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
    • H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105—After-treatment
    • H01L21/31051—Planarisation of the insulating layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/312—Organic layers, e.g. photoresist
    • H01L21/3121—Layers comprising organo-silicon compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
    • H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
    • H01L21/76819—Smoothing of the dielectric

Definitions

  • the invention relates to a process for planarizing a nonplanar surface and, more particularly, to a process for forming a planarized multilevel chip wiring structure.
  • a semiconductor chip consists of an array of semiconductor devices whose contacts are interconnected by metal patterns.
  • the metal patterns, or nets are sometimes multi-layered and separated by an insulating material, like quartz.
  • the thickness of the insulator is made sufficiently large to minimize capacitance between the different levels of wiring and also to render the insulator more tolerant to particulate defects.
  • Connections between nets are made by via studs (also known as vertical wires) which penetrate the insulator.
  • the vertical wire is formed by metal lift-off process described, for example, in U.S. Pat. No. 4,004,044 issued to Franco et al and assigned to the present assignee. The vertical wire is put in place before the insulator is deposited.
  • RIE reactive ion etching
  • ion milling the surface of the insulator is planarized and the top of the stud is exposed. Planarization is necessary since it improves the reliability of subsequent wiring levels as these wires do not have to traverse topography.
  • U.S. Patent 4,541,169 issued to Bartush and assigned to the present assignee discloses a planarization process in the context of making studs at different levels in a chip.
  • silicon dioxide layer is deposited and planarized, by etching using a thick photoresist planarization layer, to expose the most elevated studs.
  • a silicon nitride layer is then deposited and using the same mask pattern used to delineate the studs, the nitride (and the residual oxide over the the depressed studs) is etched to expose all the studs.
  • U.S. Pat. No. 4,541,168 issued to Galie et al and assigned to the present assignee discloses a method for making metal contact studs between first level metal and regions of a semiconductor device with the studs butting against polyimide-filled trenches.
  • the metal studs are formed by lift-off followed by sputter depositing silicon dioxide layer of thickness about the stud height, obtaining a nonplanar oxide structure.
  • a planarizing photoresist is applied and the resist and oxide are etched to expose the studs.
  • FIG. 1 and 2 A basic problem with these prior art methods is peak inversion. To explain, reference is made to Figs. 1 and 2 wherein a semiconductor substrate 10 having two metal studs 12 and 14 of different width is illustrated. When an insulator, such as oxide, layer 16 is deposited over the studed structure, peaks 18 and mesas 20 of oxide will be formed over the narrow and wide studs 12 and 14, respectively.
  • an insulator such as oxide
  • etch rate ratio of quartz to resist is, typically, about 1.4:1.0
  • etch rate ratio of quartz to resist is, typically, about 1.4:1.0
  • these oxide structures tend to etch off more quickly than the remainder of the oxide (which is still protected by the resist 22 thereover).
  • the peaks and mesas of the oxide are inverted as illustrated in Fig. 2.
  • the resulting structure will be of nonplanar topography consisting of an oxide medium 16 having studs 12 and 14 and vias 24 and 26. Such topography is undesirable as it leads to breakage of the next level wiring metal that is subsequently formed owing to the steepness of the vias in the oxide.
  • the wiring is prone to be fractured due to the sharp edges of the studs, leading to a low device yield and/or reliability.
  • Yet another problem is poor step coverage at the edges of the studs, which, due to electromigration, poses reliability concerns.
  • the invention is a process for planarizing a nonplanar surface.
  • a substrate having a nonplanar insulator e.g. an organosilicate such as SiO2
  • a planarizing photoactive photoresist medium is applied.
  • the photoresist is spin coated followed by soft baking at a sufficiently low temperature to drive out the solvent therein while maintaining the photoactivity of the resist.
  • the dried, photoactive resist is then silylated to convert it into a material having the same etch rate as that of the underlying insulator.
  • the conversion is accomplished by subjecting the dried resist to a silylation bath consisting of a silylating agent which can substitute SiO groups into the resist.
  • the silylating agent could be an organosilane or organosilazane. Specific examples of these agents are hexamethylcyclotrisilazane, octamethylcyclotetra- silazane, hexamethyldisilazane, N,N,dimethyl aminotri- methylsilane and N,N,diethylaminotrimethylsilane.
  • the silyation process step is accomplished at a temperature in the range 40-80°C for a period determined by the scale of 1 minute per thousand Angstroms thickness of the planarizing photoresist. Once the silyation process is complete, the resist is rendered harder and converted to SiO, while maintaining its planar surface.
  • the resulting structure is subjected to an etching step, typically, CF4 + O2 RIE or ion milling. Since the etch rate of the silylated resist is the same as that of the insulator, upon etching down to the level of the lowest valley in the insulator, the surface of insulator is made perfectly planar.
  • an etching step typically, CF4 + O2 RIE or ion milling. Since the etch rate of the silylated resist is the same as that of the insulator, upon etching down to the level of the lowest valley in the insulator, the surface of insulator is made perfectly planar.
  • the invention is a process for forming a planarized multilevel chip wiring structure.
  • an insulator e.g., quartz
  • a thick planarizing photoactive photoresist is applied.
  • the photoresist is converted by silylation to SiO material having an etch rate quite comparable to that of the quartz, while preserving its surface planarity. Unwanted portions of the silylated resist and quartz are uniformly etched back to expose the stud.
  • Figs. 1 and 2 show in cross-sectional representation successive views of a semiconductor structure having vertical wiring, pointing out the problems of the prior art planarization processes.
  • Figs. 3-5 are cross-sectional representations of a studed semiconductor structure undergoing the planarization process according to the present invention.
  • Fig. 6 is a magnified photograph of a vertical wiring structure suffering from quartz peak inversion, characteristic of the prior art.
  • Fig. 7 is a magnified photograph of a vertical wiring structure made in accordance with the present invention, without the occurrence of quartz peak inversion.
  • vertical wiring or studs designated by numerals 32 and 34 are formed by conventional process.
  • the width of the vertical wiring varies, typically, from 0.5 micrometer to 8 micrometers.
  • the vertical wiring may be, for example, in contact with elements of a semiconductor device (not shown) formed on the substrate 10.
  • the studs 32 and 34 may be formed on selected localized regions of a first level metal pattern (not shown) formed on the substrate.
  • the structure is covered with a layer 36 of an organosilicate material (i.e., a material having the SiO group) such as siloxane or silicon dioxide (quartz).
  • SiO2 may be sputtered according to standard sputtering technique. Due to conformality of layer 36, a mesa 38 and peak 40 of oxide is formed over the wide and narrow studs 32 and 34, respectively.
  • a photoactive photosensitive layer 42 is applied, as indicated in Fig. 3 to planarize the structure.
  • An example of the layer material 42 is photoactive photoresist.
  • the thickness of the photoresist layer 42 is typically 1-2.5 micrometers, the actual thickness being determined by the height of the peak 40. The higher the peak height, the thicker is the photoresist to obtain planar photoresist surface 44.
  • the photoresist is typically spin-coated, followed by soft-baking at a sufficiently low temperature to drive out the solvents therein, while maintaining the photoactivity of the photoresist.
  • the next process step is converting the resist into a material having substantially the same RIE or ion milling rate as the insulator 36.
  • This is achieved by silylating the resist 42.
  • Silylation is accomplished by subjecting the resist layer 42 to a silylation bath consisting of a silylating agent such as an organo-silazane or organosilane.
  • organosilazane are hexamethylcyclotrisilazane (HMCTS), hexamethyldisilazane (HMDS) and octamethylcyclotetrasilazane (OMCTS).
  • organosilanes are N,N,dimethyl-aminotrimethylsilane (TMSDMA) and N,N, diethylamino-trimethylsilane (TMSDEA).
  • TMSDMA N,N,dimethyl-aminotrimethylsilane
  • TMSDEA diethylamino-trimethylsilane
  • a chemical reaction occurs in which bonds are broken and SiO groups are substituted into the photoactive compound in the photoresist 42.
  • the silylation process step is accomplished at a temperature of 40-80°C. Temperatures higher than 80°C may not be suitable since then the resist 42 may begin to strip.
  • the silylation is carried out for a period of time determined by the scale of 1 minute per thousand Angstroms thickness of the resist 42. In other words, for a 1,0100 ⁇ m thick resist, silylation is complete in approximately 10 mins.
  • the direct result of the silylation process step is that the resist layer 42 is not only rendered harder, but, more importantly, converted to SiO layer 46, while maintaining the planar surface 44 of the resist.
  • the resist is converted into a material having the same etch rate as that of the quartz material 36. Since the silylated resist is virtually indistinguishable, from etching viewpoint, the previous composite layer of oxide 36 and resist 42 (Fig. 3) is transformed into a single layer of an organosilicate as indicated in Fig. 4.
  • the top surfaces of the studs 32 and 34 are exposed and the surface of the insulator layer 36 that remains will be coplanar with the exposed stud surfaces (as indicated in Fig. 5).
  • Fig. 7 is a photograph in a view taken from the top of a silicon substrate having a number of metal studs embedded in a planar quartz layer.
  • the quartz is coplanar with all the studs, regardless of their width, and free of via holes around the studs.
  • This improved result of the invention becomes particularly apparent when compared with the silicon substrate displayed in Fig. 6 which was fabricated without the silylation process of the invention, showing vividly the quartz peak inversion.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)
  • Drying Of Semiconductors (AREA)
  • Formation Of Insulating Films (AREA)

Claims (21)

  1. Einebnungsvefahren, bei welchem:
    ein Substrat mit einer unebenen Isolatoroberfläche bereitgestellt wird;
    diese Oberfläche mit einer lichtempfindlichen Schicht überzogen wird, um von dieser eine im wesentlichen ebene Oberfläche zu erhalten;
    die lichtempfindliche Schicht in ein Material umgewandelt wird, dessen Ätzrate von jener des Isolators nicht unterscheidbar ist, wobei die photo-aktiven Eigenschaften der lichtempfindlichen Schicht erhalten bleiben und das Umwandeln durch Silylierung der lichtempfindlichen Schicht erreicht wird;
    und dieses Material und Oberflächenabschnitte des Isolators geätzt werden, um die Isolatoroberfläche im wesentlichen eben zu machen.
  2. Verfahren nach Anspruch 1, bei welchem der Silylierungsprozeß umfaßt, daß die lichtempfindliche Schicht entweder einem organischen Silazan oder einem organischen Silan ausgesetzt wird.
  3. Verfahren nach Anspruch 2, bei welchem das organische Silazan aus der Gruppe ausgewählt wird, die aus Hexamethyldisilazan, Hexamethylcyclotrisilazan und Octomethylcyclotetrasilazan besteht.
  4. Verfahren nach Anspruch 2, bei welchem das organische Silan aus einer Gruppe ausgewählt wird, die aus N, N-Diethylaminotrimethylsilan und N,N Di methylaminotrimethylsilan besteht.
  5. Verfahren nach Anspruch 3 oder 4, bei welchem der Silylierungsprozeß für eine Zeit durchgeführt wird, die durch ein Ausmaß von etwa 1 Minute pro 100 µm Dicke des lichtempfindlichen Materials bestimmt ist.
  6. Verfahren nach Anspruch 3, bei welchem der Silylierungsprozeß bei einer Temperatur im Bereich von 40-80°C durchgeführt wird.
  7. Verfahren nach Anspruch 2, bei welchem weiters das lichtempfindliche Material wärmebehandelt wird, um bei Erhalten seiner Photoaktivität Lösungsmittel aus ihm zu entfernen.
  8. Verfahren nach irgend einem der vorgehenden Ansprüche, bei welche der Isolator aus einer Gruppe ausgewählt wird, die aus Siliziumdioxid und organischen Silikaten besteht.
  9. Verfahren nach irgend einem der vorgehenden Ansprüche, bei welchem die unebene Isolatoroberfläche zumindest einen vertikalen leitenden Vorsprung aufweist.
  10. Verfahren nach irgend einem der vorgehenden Ansprüche, bei welchem das Ätzen durch reaktives Ionenätzen oder Ionenfräsen durchgeführt wurde.
  11. Verfahren zur Herstellung von Vorsprüngen für die Verbindung metallisierter Schichten in verschiedenen Ebenen eines Halbleiterchips, enthaltend die folgenden Schritte:
    Bilden von leitenden Vorsprüngen in gewünschten Bereichen eines Halbleitersubstrats;
    überlagerndes Ablagern einer Isolierschicht auf dem Substrat, um die Vorsprünge zu bedecken, wobei die Isolierschicht eine unebene Oberfläche besitzt;
    Ausbilden eines einebnenden photoaktiven Mediums über der Isolierschicht, wobei dieses Medium eine im wesentlichen ebene obere Fläche besitzt;
    Umwandeln dieses Mediums in ein Material, dessen Ätzrate von jener des Isolators nicht unterscheidbar ist, wobei die photoaktiven Eigenschaften dieses Mediums erhalten bleiben und das Umwandeln durch Silylierung des photoaktiven Mediums erfolgt; und
    Rückätzen des Materials und von Teilen des Isolators, um die Vorsprünge freizulegen und um eine eingeebnete Isolatoroberfläche zu erhalten, die mit den Oberflächen der Vorsprünge koplanar ist.
  12. Verfahren nach Anspruch 11, bei welchem der Isolator Quarz ist.
  13. Verfahren nach Anspruch 12, bei welchem das Medium ein Photoresist ist.
  14. Verfahren nach Anspruch 13, bei welchem der Silylierungsprozeß beeinhaltet, daß der Photoresist einem Bad ausgesetzt wird, das entweder aus Hexamethyldisilazan, Hexamethylcyclotrisilazan, Octomethylcyclotetrasilazan, N, N-Dimethylaminotrimethylsilan oder N, N-Diethylaminotrimethysilan besteht.
  15. Verfahren nach Anspruch 14, bei welchem die Silylierung für eine Zeit durchgeführt wird, die durch ein Ausmaß von 1 Minute pro 100 µm Dicke des Photoresists gegeben ist.
  16. Verfahren nach Anspruch 15, bei welchem der Resist vor dem Silylierungsprozeß einer Wärmebehandlung bei niedriger Temperatur ausgesetzt wird, um Lösungsmittel in dem Photoresist auszutreiben.
  17. Verfahren nach Anspruch 16, bei welchem das Ätzen entweder durch reaktives Ionenätzen unter Verwendung eines CF₄ + O₂ Plasmas oder durch Ionenfräsen durchgeführt wird.
  18. Einebnungsverfahren, bei welchem:
    ein Substrat mit einer unebenen Isolatoroberfläche bereitgestellt wird;
    dieses Substrat mit einem silylisierbaren, photoaktiven Material überzogen wird, um von diesem eine im wesentlichen ebene Oberfläche zu erhalten;
    das silylisierbare photoaktive Material durch dessen Silylisierung in ein anderes Material umgewandelt wird, dessen Ätzrate von jener des Isolators nicht unterscheidbar ist, wobei die photoaktiven Eigenschaften des Materials erhalten bleiben; und
    dieses andere Material und Oberflächenabschnitte des Isolators geätzt werden, um die Isolatoroberfläche im wesentlichen eben zu machen.
  19. Verfahren nach Anspruch 18, bei welchem das silylisierbare Material lichtempfindlich ist.
  20. Verfahren nach Anspruch 19, bei welchem das lichtempfindliche Material ein Photoresist ist.
  21. Verfahren nach Anspruch 20, bei welchem die Silylierung umfaßt, daß der Photoresist entweder einem organischen Silazan oder einem organischen Silan ausgesetzt wird.
EP87112330A 1986-10-27 1987-08-25 Verfahren zur Herstellung ebener Flächen durch Silylation Expired - Lifetime EP0265619B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/923,779 US4816112A (en) 1986-10-27 1986-10-27 Planarization process through silylation
US923779 1986-10-27

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EP0265619A2 EP0265619A2 (de) 1988-05-04
EP0265619A3 EP0265619A3 (en) 1988-10-26
EP0265619B1 true EP0265619B1 (de) 1992-05-13

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US (1) US4816112A (de)
EP (1) EP0265619B1 (de)
JP (1) JPS63115341A (de)
AU (1) AU594518B2 (de)
BR (1) BR8705230A (de)
CA (1) CA1308609C (de)
DE (1) DE3779043D1 (de)

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US5981143A (en) * 1997-11-26 1999-11-09 Trw Inc. Chemically treated photoresist for withstanding ion bombarded processing

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US4723978A (en) * 1985-10-31 1988-02-09 International Business Machines Corporation Method for a plasma-treated polysiloxane coating
US4676868A (en) * 1986-04-23 1987-06-30 Fairchild Semiconductor Corporation Method for planarizing semiconductor substrates

Also Published As

Publication number Publication date
AU8013187A (en) 1988-05-05
US4816112A (en) 1989-03-28
CA1308609C (en) 1992-10-13
EP0265619A3 (en) 1988-10-26
AU594518B2 (en) 1990-03-08
JPH0565049B2 (de) 1993-09-16
DE3779043D1 (de) 1992-06-17
JPS63115341A (ja) 1988-05-19
EP0265619A2 (de) 1988-05-04
BR8705230A (pt) 1988-05-24

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